Aqueous textile treating emulsion



United States Patent 3,470,095 AQUEOUS TEXTILE TREATING EMULSION JosephJohn Pontelandolfo, Charlotte, NC, assignor to American CyanamidCompany, Stamford, Conn., a corporation of Maine No Drawing. Filed Feb.1, 1966, Ser. No. 523,913 Int. Cl. D06m 13/20 US. Cl. 252-83 6 ClaimsABSTRACT OF THE DISCLOSURE A textile treating composition comprising anaqueous emulsion of ('1) a triglyceride of higher fatty acids; (2)hydrogenated tallow fatty acid; (3) a mixed ester of glycerol, saidmixed ester having from 1 to 2 lower acyl ester moieties, the remainingester moieties being higher fatty acid moieties; and (4) an ethoxylatedcastor oil.

This invention relates to the production of textiles and relatedmaterials. The invention relates to a non-ionic textile finish and tothe production therefrom of treated fibers, staple fibers, felts,threads, cords, yarns, pellicles, filaments, fabrics and the like ofsynthetic or natural origin, or blends thereof. The textile finish isdesigned particularly for cellulosic textile materials, and blendsthereof. More particularly, this invention relates to textile finishingcompositions which impart softness to fibers, yarns and fabrics butwhich do not cause the fibers, yarns and fabrics treated with thecomposition to scorch when subjected to elevated temperatures.

The cationic textile softeners suffer from several disadvantages. Manyof the cationic softeners are waxy or gummy in nature making themdifficult to weigh or measure, to mix or disperse with other textiletreating agents, and to place in a form, such as an aqueous dispersion,which may be readily applied to textiles. For these reasons, it isdesirable to have a non-ionic softening composition capable of beingeffectively emulsified, having a high degree of storage stability, andcapable of imparting both a softness of hand and a high degree oflubricity to the material being treated.

Softness is very frequently required in textile materials, particularlyin fabrics used for clothing. The natural waxy, oily or fatty protectivecoatings of native fibers are often removed during the process ofscouring and bleaching of these fibers. The fibers generally becomeharsh when these lubricants are removed, and fabrics formed from thesefibers display an undesirable hand. In addition, certain coloringmatters are prone to impart a dryness and an unpleasantness of hand tothe fabric. Frequently, softeners are applied to fibers themselves toaid in the mechanical handling of these fibers since it iS verydifficult to spin any fiber from which the natural oils or waxes havebeen removed or, as in the case of man-made fibers, those which do notcontain a natural lubricant. Frequently, however, these treatmentsresult in the production of a relatively stiff fabric which is harsh tothe feel and less desirable commercially than fabrics possessing a softhand. As a result, the industry has resorted to the use of several typesof compounds for softening of finished fabrics and, in the case of rayontextile materials, for imparting thereto increased lubricity. Thesituations with which this invention is particularly concerned are thosein which softeners are applied to yarn or fabric as a finish inthemselves, to impart softness, smoothness, lubricity, fullness,suppleness, flexibility, and in some cases sewability as well.

There are a great many preparations available for softening textilematerials and most, if not all, of these preparations are based onlong-chain fatty or waxy comice pounds. The water-soluble soaps appearin a great many of these preparations, often for their softeningproperties as well as for their emulsifying properties. However, fabricswhich include these soaps, which are soap-fat emulsions at their normalalkaline pH, exhibit a tendency to scorch when heated to the elevatedtemperatures encountered in certain textile processing operations. Thistendency to scorch is apparently attributable to the presence of thesoap or soap-like material. At the elevated temperatures encountered,the textile softening compositions containing fats or soaps becomediscolored or scorched, thus marring the appearance of the fabric. Amongcompounds heretofore used have been the sulfonated hydrocarbons, waxes,stearates, and sulfonated oils, such as cottonseed oil, peanut oil,coconut oil and similar oil products. Additionally, in view of thecompetitive economics involved in the textile manufacturing field, someof the most widely employed softening agents have been sulfated orsulfonated tallow, and sulfated or sulfonated monoand diglycerides oftallow, cottonseed oil, coconut oil, peanut oil and other compoundscontaining the relatively long carbon chain of the higher fatty acids.The presence of these materials even in small amounts in cotton andrayon textiles has resulted in undesirable yellowing of the fabricsubsequent to heating thereof.

, Textile manufacturers do not find it economically expedient to treatonly a portion of a particular lot of fabric for the scorch resistanttextile finish. Furthermore, it is not known by the manufacturers howmuch or what part of a particular lot of fabric is to be subjected toelevated temperatures. Thus, it is desirable to have a heretoforeunavailable composition capable of adequately being emulsified andcapable of producing a softness of hand without the accompanyingproblems of being subject to scorching.

It should be noted that the adaptability of fibers, staple fibers,felts, cords, threads, yarns, pellicles, filaments, fibers, and the liketo automatic handling operations is of extreme importance in themanufacture of textiles. Modern high speed machinery techniques requirea feed of appropriate characteristics to permit uninterrupted and smoothoperation. Accordingly, lubricity, softness, electrostatic qualities,and the like, of the material being processed are intimately related tothe performance of the automatic mechanisms. Furthermore, the conditionof the feed when it is subjected to the machine operations is likewiserelated to the excellence of the final product. For example, in theknitting industry, an improperly or poorly lubricated yarn producesuneven stitches. In the spinning of yarn, a minimal amount oflubrication is essential to the production of an even yarn, free ofslubs. The problem is acute in the use of the more modern machinery,such as those employing the toe-to-top spinning process.

It is therefore an object of this invention to provide a textilesoftening composition suitable for use as a finish and characterized bya high degree of scorch resistance.

It is a further object of this invention to render scorch resistant,those textile softening finishes which norm-ally display a tendency toscorch.

It is a further object to obtain a textile softening compositioncharacterized by non-ionic components having excellent emulsioncharacteristics, having a high degree of fluidity, having a high degreeof affinity for textile materials, and being readily dispersible withother textile treating agents.

It is also a primary object of this invention to provide speciallytreated fibers, staple fibers, felt, cords, threads, yarns, pellicles,filaments, fabrics, and the like for the use in textile and relatedmanufacture which possess combined characteristics of softness,lubricity, and anti-static 3 properties which render them especiallyadaptable to machine handling.

An additional object is to obtain a process for making the compositionof this invention.

It is a further object to provide a process for treating these textilematerials with the composition of this invention.

In accordance with the present invention, it has been discovered thatthe objects of this invention are obtained by the treating of textilefibers, staple fibers, felt, cords, threads, yarns, pellicles,filaments, fabrics, and the like, so as to coat or to impregnate themwith a composition of matter comprising .(1) a glyceryl ester of afatty-acid ranging from about 9% up to about 50%, (2) a hydrogenatedmember selected from the group consisting of the higher saturated andunsaturated tallow fatty-acids ranging from (zero) up to about 12%, (3)a lower acyl glyceride of a higher fatty-acid ranging from about 14% upto about 55%, and (4) a vegetable oil ethoxylated with from about 28moles to 45 moles of ethylene oxide per mole of said vegetable oil, saidethoxylated oil ranging from about 14% up to about 75%, said percentagesbeing based on substantially dry weight of said composition. The textilematerial treated with the above described composition results in amaterial which is highly adaptable to machine operations, combining thecharacteristics of softness, lubricity, and anti-static properties. Thetreated textile material is substantially non-wetting.

As noted above, the finishing compositions of this invention may bestored and shipped in a substantially anhydrous condition, or mayalternatively be emulsified prior to shipping and storage by theaddition of water in an amount suflicient to emulsify, normally about20% or more. Subsequent to receipt of the finishing composition by thetextile treating manufacturer, additional water may be added to thecomposition sufficient to prepare a dilution having the characteristicswhich might be preferred for the particular material to be treated.

Accordingly, the aqueous composition of the above finishing materialcontains water ranging from about 20% to about 83%, glyceryl esterranging from about 4% to about 11%, the hydrogenated member ranging from0 to about 2% (preferably about 0.1% up to about 1.5% the glycerideranging from about to about 12%, and the ethoxylated oil ranging fromabout 6% to about 30%, where the percentages are based on the weight ofthe total aqueous composition.

It has been additionally found that the ethoxylated vegetable oil (suchas castor oil) may be effectively supplemented by the presence of apolyalkylene glycol ester ranging from an amount suflicient to beeffective up to about 2% of the aqueous composition, normally from about0.1% up to about 1.5 to obtain the textile material of hand superior tothat heretofore obtainable. The preferred polyalkylene glycol esterincludes polyethylene glycol (1000) monostearate as at least a majorcomponent of the polyethylene glycol esters employed.

The glycerol esters of the fatty acid which may be employed includecompounds of substantially similar structure such as glyceryltristearate, glyceryl trilaurate, glyceryl trimyristate, glyceryloleate, glyceryl palrnitate, glyceryl heptanoate, glyceryl caprylate,and the like. The glyceryl ester of the fatty acid which obtains thesuperior and therefore the preferred results of this inventioncritically includes glyceryl tristearate as at least a major componentof the glyceryl esters employed. Similarly, the hydrogenated memberwhich obtains the preferred results critically includes stearic acid asat least a major component of the hydrogenated members employed, othertypical hydrogenated members including acids such as lauric acid,myristic acid, oleic acid, and the like. It should be noted, however,that superior results can be expected from the saturated fatty acids.Although the aceto glycerides are critical to obtain the preferredresults of this invention, it is additionally within the scope 4 of theinvention to employ other lower acyl glycerides of a higher fatty acidsuch as formoglycerides of the higher fatty acid. It should be notedthat one of the more critical components of this invention is thevegetable oil ethoxylated with from about 28 moles to 45 moles ofethylene oxide per mole of the vegetable oil. The preferred results areobtained when the vegetable oil is castor oil. However, less effectivesubstitutes therefor include ethoxylated peanut oil, ethoxylated coconutoil, and the like.

The preferred finishing composition which obtains superior resultsemploys a vegetable oil ethoxylated with from about 35 moles to about 41moles of ethylene oxide.

Additionally, it should be noted that the above described lower acylglyceride of a higher fatty-acid is highly critical, in order to obtainthe desired properties of the composition of this invention. Thepreferred results are obtained by the employment of a glyceride whichincludes glyceryl distearate-acetate as at least a major component ofthe glycerides employed. Other glycerides, less effective, however,typically include glyceryl stearate-diacetate.

For any of the above described components, the finishing composition ofthis invention may be used alone or in admixture with othersubstantially equivalent components of the type described above.

The preferred composition for application to textile materials includesglyceryl tristearate ranging from about 8% to about 10%, the stearicacid ranging from about 0.5% to about 1.5%, the glyceryldistearate-acetate ranging from about 6% to about 8%, the ethoxylatedvegetable oil present in at least 8%, and the balance being water aloneor in combination with another suitable solvent.

Both a characteristic of the finishing composition, as well as anadvantage over prior compositions, is a low viscosity,characteristically a viscosity as low as about 19 centipoises at about25% solids, and a very small particle size, substantially all particlesbeing of a particle size below about 1 micron.

When the above composition is applied to textile material such ascotton, or a blend of cotton, or any of the other textile materialsdiscussed above as within the scope of this invention, a new compositionresults, such as a textile material characterized by softness of handand a lubricity discussed above.

Also, by the employment of the above composition as defined, a highlydesirable and workable process for applying said composition to textilematerials results from the highly emulsified composition in the aqueoussolvent, which ordinarily is only water.

Also, by the employment of the above composition of this invention, theproblems of poor stability have been substantially overcome.

It should be noted that an advantage of the composition of thisinvention lies in the ability to obtain a uniform softening of the yarn,as a result of the even distribution obtainable from the high qualityemulsion of particles less than 1 micron in size. Another advantageouscharacteristic of the finishing composition of this invention is that itis highly soluble in either warm or cold water, thereby allowing it tobe mixed at room temperature without bothersome, expensive, and timeconsuming heating up to obtain solution. The finishing compositionresists both yellowing and odor development, and is nonchlorineretentive. Additionally, it is possible to have a high solids contentwhich is characteristically higher than the normal solid content for anon-ionic liquid textile softener of this type, thereby resulting in asavings to the customer since the customer will be shipped more realproduct and less Water. Additionally, the product is very fluid, theviscosity thereby permitting easy pumping, metered measuring out of bulkstorage, and no substantial change in viscosity Between temperatures ofabout 40 F. and F. The finishing composition of this invention is anon-ionic textile softener which can be used in thermosetting resinformulations, or as a pure finish to provide soft handle and lubricationto fabric or yarn which may thereby possess enhanced physical propertiessuch as better draping qualities, better resistance to abrasion, reducedneedle cutting, and the like.

The components of the finishing composition of this invention may beadmixed in any conventional manner. However, to obtain the preferredcomposition, and to ascertain that composition has the preferredproperties discussed above, it is critical to admix the components andto obtain a temperature of at least about 85 C., preferably at leastabout 89 C. for about 2 minutes to about an hour, preferably for aboutten to about thirty minutes, followed by a prompt reduction oftemperature to below about 30 (3., preferably below about 25 C.Thereafter the composition may be bottled and labelled.

A typical composition of this invention includes 8 parts of a glycerolester of a fatty acid, one part of a hydrogenated member selected fromthe group consisting of the higher saturated and unsaturated tallowfatty acids, 8 parts of a lower acyl glyceride of a higher fatty acid, 8parts of a vegetable oil ethoxylated with from about 28 moles to about45 moles of ethylene oxide per mole of vegetable oil, and about 75 partsof water.

Another typical composition includes the components as set forth in thepreceding paragraph, except that the ethoxylated vegetable oilemulsifier is present in about 6 parts, and the composition additionallyincludes about 2 parts of a polyalkylene glycol ester such aspolyethylene glycol (1000) monostearate.

It should be noted that the aqueous composition employed in the processof treating a textile material rarely would contain more than 40% solidsbecause solids content above 40% exhibits increased viscosity to such anextent that the ratio of expensive emulsifier to the other componentsbecomes too great for the product to remain commercially feasible.

The following examples serve only to illustrate the invention disclosedherein, and do not limit the scope of the invention except as limited inthe appended claims.

EXAMPLE I The components are admixed in a vessel, and heated to 89 C.with agitation for about twenty minutes, after which the mixture isquickly cooled to about 25 C. The composition includes 8 parts ofglyceryl tristearate, 4.2 parts of stearic acid, 3.8 parts of diethyleneglycol monostearate, 8 parts of polyethylene glycol (1,000)monostearate, and 76 parts of water. The composition is illustrated inTable I. The product obtained is initially fluid but sets to a pastewithin a few days, thereby exhibiting a poor stability.

Further experiments along this line fail to give satisfactory results.

EXAMPLE II The method of admixing components is the same as that forExample I. The components employed are 7 parts of polyethylene glycol(1000) monostearate, 13 parts of acetoglyceride and 80 parts of water.

The example is repeated employing acetoglyceride made from filteredtallow. Each of the above composi tions are given an applicationevaluation on fabric and the results indicate that each had improvedhand, scorch and yellowing characteristics as compared to a standardconventional softener, but each of the above compositions set-up whenplaced in storage thereby demonstrating poor stability.

EXAMPLE III The composition is admixed according to the procedure ofExample I. The composition includes 8 parts of glyceryl tristearate, 2parts of stearic acid, 8 parts of acetoglyceride, and as emulsifierpolyethyleneoxy ethanol in varying parts, the balance being water. Anemulsion is not obtainable, demonstrating that the particular emulsifieris critical to the composition.

6 EXAMPLE IV Part A.The composition components are admixed by theprocess described in Example I. The components include 6 parts ofglyceryl tristearate, 1 part of stearic acid, 10 parts of glyceryldistearate-acetate, 8 parts of ethoxylated castor oil, and the balanceof water. The composition has a good appearance, and is illustrated inTable I below. The composition, employing 6 parts of glyceryltristearate and 10 parts of glyceryl distearateacetate, illustrates thatan acceptable composition of this invention may be prepared employing aslow as the 6 parts of the glyceryl ester of the fatty-acid, andillustrates that 10 parts of the lower acyl glyceride of a higherfattyacid may be employed to obtain a satisfactory composition.

Part B.The composition of this invention is admixed according to Part A,except 4 parts of glyceryl tristearate is employed, and 12 parts ofglyceryl distearate-acetate is employed. The composition is viscous,thereby demonstrating the lower limit of parts that can be employed of aglyceryl ester of a fatty-acid, and demonstrating the upper limit of 12parts of a lower acyl glyceride of a higher fatty-acid.

EXAMPLE V The components are admixed according to Example I. Thecomponents include 11 parts of glyceryl tristearate, 1 part of stearicacid, 5 parts of glyceryl distearate-acetate, 8 parts of ethoxylatedcastor oil, and the balance of water. The composition has a very goodappearance and is illustrated in Table I below. This compositiondemonstrates that 11 parts or more of a glyceryl ester of a fatty-acidmay be employed to obtain a satisfactory composition of this invention.The example also illustrates the successful employment of as low as 5parts of a lower acyl glyceride of a higher fatty-acid.

EXAMPLE v1 The composition is admixed according to Example 1. Thecomponents of the composition include 8 parts of glyceryl tristearate, 2parts of stearic acid, 7 parts of glyceryl distearate-acetate, 8 partsof ethoxylated castor oil, and the remainder of water. The compositionhaving good characteristics result, and is illustrated in Table I below.The composition of this example illustrates the upper limit of theamount of hydrogenated members selected from the group consisting of thehigher saturated and unsaturated tallow fatty-acid which may be present.

EXAMPLE VII Part A.The components of the composition are admixedaccording to Example I. The components include 8 parts of glyceryltristearate, 3 parts of stearic acid, 6 parts of glyceryldistearate-acetate, 8 parts of ethoxylated castor oil and the remainderof water. The composition so prepared is a paste and is accordinglyunsatisfactory for the conventional treatment of a textile material,thereby demonstrating that 3 parts of the hydrogenated member exceed themaximum number of permissible parts, if an acceptable composition ofthis invention is to be obtained.

Part B.The composition is admixed according to Example I. The componentsinclude 8 parts of glyceryl tristearate, 4 parts of stearic acid, 5parts of glyceryl distearate-acetate, 8 parts of ethoxylated castor oil,and the remainder of water. The composition thereby prepared sets,thereby illustrating an unacceptable composition, employing thehydrogenated number in excess of the maximum allowable for purposes ofthis invention.

EXAMPLE VIH Part A.The composition is admixed according to Example I.The components include 11 parts of glyceryl tristearate, 6 parts ofglyceryl distearate-acetate, 8 parts of ethoxylated castor oil, and theremainder of water. The composition resulting was good, and isillustrated in Table 3,470,095 7 8 I below. This compositiondemonstrates that the comtrating this invention are intended to limitthe invention position of this invention need not necessarily include aonly insofar as stated in this specification and as the folhydrogenatedmember selected from the group consisting lowing claims are limited. ofthe higher saturated and unsaturated fatty-acids. I claim:

Part B.The composition is admixed according to 5 1. A textile treatingcomposition consisting essentially Example I. The components include 9parts of glyceryl of an aqueous emulsion of (1) from about 4 to 11% oftristearate, 8 parts of glyceryl distearate-acetate, 8 parts atriglyceride of higher fatty acids; (2) from about to of ethoxylatedcastor oil, and the remainder of water. 2% of a hydrogenated tallowfatty acid; (3) from about The composition is very excellent and furtherdemonto 12% of a mixed tri ester of glycerol, said mixed ester stratesthe composition of this invention in the absence having from 1 to 2acetyl ester moieties, the remaining of a hydrogenated member selectedfrom the group conester moieties being higher fatty acid moieties; (4)from sisting of the higher saturated and unsaturated tallow about 6 to30% of an ethoxylated castor oil, ethoxylated fatty-acid, as well asillustrating the use of a smaller with from about 28 to 45 mols ofethylene oxide per mol amount of glyceryl tristearate than was employedin Part of castor oil; and (5) from about 20 to 83% water said A of thisexample, Part A employing the maximum of percentages being based on theWeight of the total compermissible glyceryl ester of the fatty-acid.position.

EXAMPLE IX 2. A compositionaccording to claim 1, in which saidethoxylated castor oil 1s present in an amount of at least Part A.--Thecomponents were admixed in the manner about 8% by weight, saidtriglyceride comprises glyceryl described in Example I. The componentsinclude 10 parts t i t t present f about 3% t about 10% b 0f gly ryltristeafate, 8 Parts Of g y ry distearate-aceweight, said hydrogenatedmember comprises stearic acid tale, 7 Parts of lf q P f the remainderpresent from about 0.5% to about 1.5% by weight, said of W TheCOmPOSItIOII 0f U11S lllvfilltlon thereby P mixed ester comprisesglyceryl distearate-acetate present duced is excellent, and demonstratesthe employment of from b t 6% t b t 8% by weight, aid a t oil a higheram of g y y ester of a fattv-aid,the1ack is ethoxylated with from about35 to about 41 moles of Of y hydrogenated member of a Saturated orunsatur' ethylene oxide, said water is present in an amount of at rateda yt 3 Sma11er amunt of ethoxylated least about 57% by weight, and saidcomposition is noncastor 011 than used in the foregoing examples. i0niPart B.The components of the composition are ad- A composition accordingto claim 1, including a mixed according to the method described inExample I. The components include 10 parts of glyceryl tristearate, 1part of stearic acid, 5 parts of glyceryl distearate-acetate, 9 parts ofethoxylated castor oil, and the remainder of water. The compositionproduct of this invention thereby produced is excellent and demonstratesthe employment of the lower limit of the amount of a lower acylglyceride of a higher fatty-acid which may be employed and also Processtreatmg teiftlle l compnsmg illustrates the employment of a higheramount of ethoxylapplylng a cfmlposltlon to a textlle materlal an amountated castor oil than employed in any of the foregoing sufficient to1mpart 3. softness Of hand and a degree polyethylene glycol monostearateranging up to about 2% based on the weight of said aqueous composition.

4. A composition according to claim 1 having a viscosity of as low as atleast about 19 centipoises at about 25% solids, and having individualparticle sizes substantially all below about one micron.

examples, of lubricity to said material, said composition being de- Eachof the above examples are illustrated in Table I fined according toclaim 1. below: 6. A textile material characterized by a softness ofTABLE I Parts per 100, by weight Example No 1 2 3 4A 4B 5 6 7A 7 B 8A813 9A 9B Glyceryl tristearate 8 6 4 11 8 8 8 Stearic acid 4. 2 2 1 1 12 3 4 Glyceryl distearate-acetate 13 8 10 12 5 7 6 5 Ethoxylated castoroil--- 8 8 8 8 8 8 Water 76 80 var 75 75 75 75 75 75 Polyethylene glycol(1,000) monostearate-. 8 7 Polyethyleneoxyl ethanol (emulsifier) var.Diethylene, glycol monostearate 3.8 Appearance Poor Poor Poor Good Vrs.00d pH l 4. 38 4. 40 4. 52 4.

No satisfactory emulsion possible. Viscous. Very good. Very excellent.

EXAMPLE X hand and a high degree of lubricity comprising a textilematerial having distributed thereon a composition ac- Employmg thegeneral procedure of Example I, the cording to claim L composition ofthis invention is again prepared as follows:

The reactor vessel is charged with about 7500 lbs. of References cuedwater, after which about 900 lbs. of the emulsifier (such UNITED STATESPATENTS as ethoxylated castor oil) of this invention is charged,2,005,785 6/1935 Hibb t r 1 252 3,6 X after which about 900 lbs. ofhydrogenated tallow gly- 2,238,882 4/1941 Goodings et al. 2528.6 ceride(such as glyceryl tristearate) is charged, after 2,456,283 12/1948 J ffon 2528.9 X which about 100 lbs. of hydrogenated tallow fatty acid2,978,408 4/1961 Lanner t 1 252 8,6 X is charged, and after which about600 l s. of a g y- 3,039,895 6/1962 Yuk 2528.6 X cerides (such asglyceryl distearate acetate is g 3,170,876 2/1965 Olney 2528.9 X Theagitator is run at highest speed and the r a t atch 3,198,732, 8/1965Olney 2528.9 is heated to about 88-90 C., and is held at about 90 C.3,306,850 2/1967 Olsen 2528.9 X for about 20 minutes, followed bycooling the batch to about 25 C. HERBERT B. GUYNN, Primary Examiner Itis within the scope of this invention to make such modifications of thecomposition and process described above as would be obvious to a personof ordinary skill 117 139.5. in this art, and it is understood that theexamples illus-

